高效液相色谱法测定稻田土壤中环吡氟草酮残留

Study on residue analysis of flufenacet in rice soil

建立了高效液相色谱法测定稻田土壤中环吡氟草酮的分析方法。比较了不同的色谱柱、流动相组成及提取溶液对分析结果的影响。确定优化的色谱条件为：Waters Atlantis T_3色谱柱（4.6 mm×250 mm,5μm）,乙腈-磷酸水（体积分数0.02%）（V/V=50：50）为流动相,流速1 mL/min,柱温30℃,进样量20μL;PDA检测器,检测波长270 nm。确定了土壤样品中目标物的提取方法：酸化乙腈提取,高速离心机分离出提取液,经盐析分液净化,旋转蒸发仪浓缩、定容。结果表明,环吡氟草酮在0.1~20.0 mg/L质量浓度范围内呈良好线性关系,线性相关系数r≥0.999;仪器检出限为0.02 mg/L。添加回收试验结果表明,方法的回收率为78.0%~88.6%,相对标准偏差（n=6）为0.90%~1.0%,方法检出限为0.005 mg/kg。该方法可应用于实际样品检测。

A method for the determination of flufenacet in rice soil was established by high performance liquid chromatographic （HPLC）. The effect of chromatographic column types, and also extraction solution types on the analysis results were studied comparab mobile phases types, ly in the paper. The optimum HPLC conditions were confirmed as follows： separation column： Waters Atlantis T3 chromatographic column （4. 6 mm × 250 mm, 5 μm） , mobile phase ： aeetonitrile and 0. 02% phosphate aqueous solution （ V/V = 50 ： 50 ） , flow rate ： 1 m/min, column temperature ： 30℃ and injection volume： 20μL, PDA detector wavelength： 270 nm. The extraction process was as follows：soil samples were extracted with acidified acetonitrile for twice, and the extract was salted out and purified by liquid-liquid distribution. Afterwards, the organic phase was condensed and analyzed by HPLC. Under the optimized conditions, the calibration curves of flufenacet showed good linearities in the range of 0. 1 -20. 0 mg/L mass concentration, with correlation coefficients higher than 0. 999. The instrumental detection limit of flufenacet was 0. 02 mg/L. The spiked recoveries were in the range of 78.0% - 88.6% with RSDs（ n = 6） of 0. 9% - 1.0%, and the detection limits was 0. 005 mg/kg. With the advantages of convenience in operation, excellent separation on capability, high sensitivity and accuracy, the proposed method was successfully applied to the determination of flufenaeetin in real soil samples.